先驱体法制备非晶态SiCNO材料
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摘要
以甲基乙烯基二氯硅烷、乙烯基三氯硅烷、氨基甲酸铵和环己烷作为原料,通过溶剂热合成路线制备出SiCNO陶瓷的液态先驱体。先驱体经1100℃热解后,转变为非晶态SiCNO材料。FT-IR红外分析显示先驱体中含有异氰酸酯官能团。非晶态SiCNO具有良好的高温热稳定性,在1500℃时仍保持无定形状态,1600℃以上时基体中析出Si2N2O和少量的β-SiC相。
Liquid SiCNO precursor was prepared by a solvo-thermal route with ammonium carbanate,methyl vinyl dichlorosilane and vinyl triclorosilicane as raw materials.The amorphous SiCNO was then obtained through the pyrolysis of the liquid precursor around 1100℃.FT-IR analysis indicated that there are isocyanate groups in the precursor.The amorphous SiCNO has favorable thermal stability without any decompositiontill 1500℃.However,at temperature above 1600℃ Si2 N2 O andβ-SiC crystalline phases start to precipitate out of the amorphous matrix.
Liquid SiCNO precursor was prepared by a solvo-thermal route with ammonium carbanate,methyl vinyl dichlorosilane and vinyl triclorosilicane as raw materials.The amorphous SiCNO was then obtained through the pyrolysis of the liquid precursor around 1100℃.FT-IR analysis indicated that there are isocyanate groups in the precursor.The amorphous SiCNO has favorable thermal stability without any decompositiontill 1500℃.However,at temperature above 1600℃ Si2 N2 O andβ-SiC crystalline phases start to precipitate out of the amorphous matrix.
引文
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[4]张长瑞,郝元恺.陶瓷基复合材料[M].长沙:国防科技大学出版社,2001,273~302.
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[6]张磊,赵东林,沈曾民.聚碳硅烷和二乙烯基苯的交联及纳米SiC陶瓷的制备[J].材料科学与工程学报,2009,27(3):421~425.
[7]范雪骐,陈来,吴市,等.聚甲基硅烷/二乙烯基苯的交联和裂解[J].材料科学与工程学报,2006,24(6):920~922.
[8]H.J.Seifeit,J.Q.Peng,H.L.Lukas.Phase Equilibria and Thermal Analysis of Si-C-N Ceramics[J].J.Alloys Compd.,2001,320:251~261.
[9]C.Moysan,R.Riedel,R.Harshe,T.Rouxel,F.Augereau.Mechanical characterization of a polysiloxane-derived SiOC glass[J].J.Eur.Ceram.Soc.,2007,27:397~403.
[10]徐天恒,马青松,陈朝辉.聚硅氧烷转化SiOC陶瓷微观结构的研究进展[J].材料科学与工程学报,2010,28(5):773~777.
[11]L.Bois,J.Maquet,F Babonneau,et al.[J].Chem.Mat.,1994,6:796~802.
[12]D.Seyferth.Synthesis of Some Organosilicon Polymers and Their Pyrolytic Conversion to Ceramics[M].1989,224:525~527.
[13]陈蒲生,张昊,冯文修,刘剑,刘小阳,王锋.PECVD法低温形成SiO_xN_y介质膜的俄歇电子能谱和红外吸收光谱分析[J].Semiconductor Technology,2002,27(7):73~76.
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[15]Y.kamimura,O.Haba,T.Endo.Latent reactive polymers containing isocyanate moiety that show extreme stability under aerobic atmosphere[J].J.Polym.Sci.,Part A:Polym.Chem.,2006,44:2448~2453.
[16]H.Tietz,O.Rademacher,G.Zahn.A Novel Isocyanate Reaction The Formation and Structure of Unexpected Cycloadducts[J].Eur.J.Org.Chem.,2000,2105~2112.
[17]E.Q.Xie,Z.W.Ma,H.F.Lin,Z.M.Zhang,D.Y.He.Preparation and characterization of SiCN films[J].Opt.Mater.,2003,23:151~156.
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[19]C.W.Chen,C.C.Huang,Y.Y.Lin,L.C.Chen,K.H.Chen.The affinity of Si-N and Si-C bonding in amorphous silicon carbon nitride(a-SiCN)thin film[J].Diamond Relat.Mater.,2005,14:1126~1130.
[20]K.Yamamoto,Y.Koga,S.Fujiwara.XPS studies of amorphous SiCN thin films prepared by nitrogen ion-assisted pulsed-laser deposition of SiC target[J].Diamond Relat.Mater,2001,10:1921~1926.